Determination of 23 Metal Elements in Detailed Soil Survey Samples by Inductively Coupled Plasma-Mass Spectrometry with Three Acid Stepwise Digestion
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摘要: 土壤详查样品具有数量大、基质复杂、有机质含量高的特点，传统上采用多种混合酸体系的消解方法，不仅会造成有机质消解不完全，消解后的溶液中常有黑色的碳质存在，而且样品消解后只用稀硝酸提取，一些难溶氧化物、硫酸盐、氟化物难以形成可溶性盐，致使提取不彻底，若用逆王水提取则易大量引入氯离子造成氯的多原子离子质谱干扰。本文针对上述问题，充分利用硝酸、氢氟酸、高氯酸的不同特性，采用电热板控温，三酸分步加入法消解土壤样品，对于消解后的样品，采用硝酸-盐酸（体积比20：1）作为提取剂，有效降低了氯的多原子离子质谱干扰且提取彻底。结果表明：本方法能够消解土壤中有机质和硅酸盐组分，具有试剂用量少、氯的质谱干扰小、操作流程简单、工作效率高等优点，方法检出限（3s）更低（0.0008~0.90mg/kg）。将该方法应用于暗棕壤、石灰岩土壤、黄棕壤国家标准物质中23种元素的测定，其测定结果明显优于传统的消解方法，相对标准偏差（RSD，n=6）为0.022%~5.83%，相对误差为-8.33%~9.17%，测定时与认定值相符。该方法具有较高的适用性和可靠性。
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关键词:
- 土壤详查样品 /
- 金属元素 /
- 硝酸-氢氟酸-高氯酸消解 /
- 电感耦合等离子体质谱法
Abstract:OBJECTIVES The soil detailed survey samples have the characteristics of large quantity, complex matrix, and high organic matter content. The traditional digestion method using a variety of mixed acid systems not only leads to incomplete digestion of organic matter, but also leaves black carbon in the solution after digestion. Because the sample is only extracted with dilute nitric acid, some insoluble oxides, sulfates, and fluorides are difficult to form soluble salts, resulting in incomplete extraction. If the reverse aqua regia is used during extraction, it is easy to introduce a large amount of chloride ions and cause the interference problem of chlorine multi-atomic ion mass spectrometry. OBJECTIVES In order to accurately determine 23 metal elements in soil. The analysis efficiency and quality can be improved by making full use of the different characteristics of nitric acid, hydrofluoric acid and perchloric acid in sample digestion. METHODS Soil samples were digested on electric heating plate, by stepwise addition of nitric acid, hydrofluoric acid and perchloric acid. For the digested samples, nitric acid-hydrochloric acid (20:1, V/V) mixed solution was used as the extractant, effectively reducing the interference of chlorine polyatomic ion mass spectrum and extracting elements thoroughly. Twenty-three metal elements in the soil were simultaneously determined by inductively coupled plasma-mass spectrometry (ICP-MS). RESULTS This method can effectively digest organic matter and silicate components in soil. It has the advantages of less reagent consumption, less mass spectrum interference of chlorine, simple operation process, high working efficiency, and lower detection limit (0.0008-0.90mg/kg, 3s). This method was applied to the national level standard substance such as dark brown soil, limestone soil, yellow brown soil samples for the determination of 23 elements, and the measurement result was superior to the traditional digestion method. The precision (RSD, n=6) was 0.022%-5.83% and relative error was -8.33% to 9.17%. The results are consistent with the certified values, indicating that the method is applicable and reliable. CONCLUSIONS The method for the simultaneous determination of 23 elements in soil samples by ICP-MS with three acid stepwise digestion has high applicability and reliability. -
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表 1 多元素标准溶液
Table 1. Standard solution of multiple elements
样品编号 多元素组合浓度(μg/L) Cd、In Li、Cu、Pb、Zn、Cr、Ni、Ⅴ、As Be、Mo、Tl Co、Ga、W、Cs、Sb、Bi Mn、Ba Sn Sr 1-1 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1-2 0.010 2.00 0.10 0.50 25.0 0.25 10.0 1-3 0.020 4.00 0.25 1.00 50.0 0.50 20.0 1-4 0.050 8.00 0.50 2.00 100 1.00 40.0 1-5 0.10 10.0 0.75 5.00 200 1.50 60.0 1-6 0.20 20.0 1.00 10.0 300 2.00 80.0 1-7 0.50 40.0 1.50 15.0 400 2.50 100 1-8 1.00 80.0 2.00 20.0 500 3.00 150 1-9 2.00 100 2.50 25.0 600 4.00 200 1-10 3.00 120 3.50 30.0 800 6.00 300 1-11 4.00 160 4.00 35.0 1000 8.00 400 1-12 5.00 200 5.00 40.0 1200 10.0 500 
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表 2 土壤标准物质GBW07454中23种金属元素的测定结果
Table 2. Analytical results of 23 metallic elements in the GBW07454 soil reference material
待测元素 认定值(mg/kg) 12次测定平均值(mg/kg) RSD(%) 7Li 32±2 30.3 5.01 9Be 1.9±0.1 1.85 3.25 51Ⅴ 77±4 79.6 1.08 52Cr 66±4 66.7 3.36 55Mn 632±21 615 1.59 59Co 12±0.5 11.8 0.67 60Ni 30±1 29.4 1.98 65Cu 23.6±1.0 24.5 4.13 66Zn 66±2 67.9 3.38 71Ga 14.9±0.4 15.1 0.32 75As 12.9±0.5 13.8 6.08 88Sr 192±6 197 1.86 98Mo 0.72±0.07 0.77 2.79 114Cd 0.175±0.01 0.172 3.54 115In 0.049±0.005 0.048 7.37 118Sn 2.9±0.4 3.05 3.44 121Sb 1.13±0.05 1.16 4.95 133Cs 7.2±0.3 6.98 1.99 137Ba 495±16 502 1.06 182W 8.3±0.5 8.56 6.06 205Tl 0.59±0.06 0.57 3.81 208Pb 22±1 21.8 0.98 209Bi 0.32±0.01 0.31 4.85
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表 3 本方法和标准方法的检出限对比
Table 3. Comparison of detection limits between this method and standard method
元素 检出限(mg/kg) 本方法 标准方法 Li 0.026 0.06 Be 0.004 0.006 Ⅴ 0.79 3 Cr 0.20 2 Mn 0.14 0.2 Tl 0.001 0.003 Co 0.005 0.02 Ni 0.08 0.6 Cu 0.32 0.6 Zn 0.90 1.1 Ga 0.07 0.1 Pb 0.22 0.003 As 0.25 - Sr 0.30 0.4 Mo 0.005 0.02 Cd 0.003 0.021 In 0.0008 0.002 Bi 0.009 0.015 Sn 0.02 - Sb 0.01 0.02 Cs 0.002 0.003 Ba 0.95 1.1 W 0.006 0.02
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表 4 本方法和标准方法的实验条件对比
Table 4. Comparison of experimental conditions between this method and standard method
对比项目 本文方法 标准方法 取样量 0.1000g 0.2500g 耗酸量 硝酸5mL，氢氟酸4mL，高氯酸1mL 硝酸10mL，氢氟酸15mL，高氯酸3mL 样品处理时间 3h左右 25h以上 消解步骤 针对土壤样品特点，三酸分三步控温加入 分两次加入三种混合酸，各种酸的利用效率低 提取方法 硝酸-盐酸(20:1，体积比)并用水稀释一倍溶液5mL提取 加王水8mL蒸发至2~3mL提取，Cl-浓度高 溶液稀释 定容至100mL容量瓶中，无稀释 定容至25mL试管中，稀释10倍
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表 5 方法精密度和准确度
Table 5. Precision and accuracy tests of the method
元素 GBW07401 GBW07403 GBW07404 认定值(mg/kg) 测定平均值(mg/kg) RSD(%) 相对误差(%) 认定值(mg/kg) 测定平均值(mg/kg) RSD(%) 相对误差(%) 认定值(mg/kg) 测定平均值(mg/kg) RSD(%) 相对误差(%) 7Li 35±1 34.1 1.31 -3.22 18.4±0.8 18.7 0.47 4.73 55±2 54.2 1.08 -1.61 9Be 2.5±0.3 2.42 2.57 -3.20 1.4±0.3 1.44 3.68 2.86 1.85±0.34 1.97 1.52 6.49 51Ⅴ 86±4 85.6 1.06 -0.47 36±4 38.2 2.49 6.11 247±14 241 1.36 -2.43 52Cr 62±4 62.5 1.03 0.81 32±6 31.0 0.87 -3.13 370±16 366 0.27 -1.08 55Mn 1760±63 1721 2.49 -2.22 304±21 296 2.55 -2.63 1420±75 1405 1.34 -1.06 59Co 14.2±1.0 13.9 0.79 -2.11 5.5±1.0 5.74 2.02 4.36 22±2 20.9 1.46 -5.00 60Ni 20.4±1.8 21.3 0.09 4.41 12±2.7 13.1 0.09 9.17 64±5 64.3 0.04 0.47 65Cu 21±2 20.7 0.05 -1.43 11.4±1.6 10.9 0.04 -4.39 40±3 39.7 0.05 -0.75 66Zn 680±25 675 0.02 -0.74 31±4 32.9 0.04 6.13 210±13 215 0.04 2.38 71Ga 19.3±1.1 18.9 1.05 -2.07 31±5 31.3 0.84 0.73 31±3 31.7 1.19 2.26 75As 34±4 32.3 2.56 -5.00 4.4±0.9 4.68 3.87 6.36 58±6 59.1 1.23 1.90 88Sr 155±7 158 0.08 1.94 380±25 369 0.06 -2.89 77±6 79.4 1.25 3.12 98Mo 1.4±0.1 1.46 2.78 4.29 0.31±0.13 0.33 5.83 6.45 2.6±0.3 2.59 1.61 -0.38 114Cd 4.3±0.4 4.43 0.06 3.02 0.06±0.022 0.058 0.05 -3.33 0.35±0.06 0.37 0.09 5.71 115In 0.08±0.02 0.082 0.03 2.50 0.031±0.03 0.029 0.10 -6.45 0.12±0.03 0.11 1.06 -8.33 118Sn 6.1±0.7 6.03 1.77 -1.15 2.5±0.4 2.59 3.60 3.60 5.7±0.9 5.95 1.92 4.39 121Sb 0.87±0.21 0.82 0.92 -5.75 0.44±0.08 0.47 1.58 6.82 6.3±1.1 6.17 2.36 -2.06 133Cs 9±0.7 8.87 0.43 -1.44 3.2±0.4 3.25 0.88 1.56 21.4±1.0 19.8 0.29 -7.48 137Ba 590±32 599 0.10 1.53 1210±65 1187 0.03 -1.90 213±20 220 1.43 3.29 182W 3.1±0.3 3.21 3.68 3.55 0.96±0.12 1.04 4.85 8.33 6.2±0.5 6.09 2.07 -1.77 205Tl 1.0±0.2 1.02 1.96 2.00 0.48±0.05 0.5 2.50 4.17 0.94±0.25 0.97 2.25 3.19 208Pb 98±6 98.8 0.03 0.82 26±3 26.2 0.06 0.77 58±5 57.4 0.06 -1.03 209Bi 1.2±0.1 1.17 2.78 -2.50 0.17±0.03 0.18 4.62 5.88 1.04±0.13 0.99 3.82 -4.81
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